CN113957274A - Vanadium-aluminum alloy and preparation method thereof - Google Patents

Vanadium-aluminum alloy and preparation method thereof Download PDF

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CN113957274A
CN113957274A CN202111121138.3A CN202111121138A CN113957274A CN 113957274 A CN113957274 A CN 113957274A CN 202111121138 A CN202111121138 A CN 202111121138A CN 113957274 A CN113957274 A CN 113957274A
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vanadium
aluminum alloy
mixture
aluminum
preparing
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陈海军
尹丹凤
高雷章
师启华
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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Pangang Group Panzhihua Iron and Steel Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/04Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02Alloys based on vanadium, niobium, or tantalum
    • C22C27/025Alloys based on vanadium, niobium, or tantalum alloys based on vanadium

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  • Engineering & Computer Science (AREA)
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  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to the field of metallurgy and discloses a vanadium-aluminum alloy and a preparation method thereof. The method comprises the following steps: (1) mixing vanadium pentoxide and aluminum particles according to the weight ratio of (1.03-1.9) to 1 to obtain a mixture; (2) and paving part of the mixture at the bottom of the smelting furnace, igniting and igniting the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to perform aluminothermic reaction, and standing after the reaction is finished to obtain the vanadium-aluminum alloy. Compared with the prior art, the preparation method provided by the invention has the advantages that the production scale can be enlarged by adopting a continuous feeding mode, the alloy ingot can be kept in a molten state for a longer time, and the yield of vanadium is improved. And conventional lime and other slagging coolants are not added to adjust heat, so that the cost is lower, the introduction of impurities can be reduced, the content of the impurities in the vanadium-aluminum alloy can be further reduced, and the purity of the obtained alloy is higher.

Description

Vanadium-aluminum alloy and preparation method thereof
Technical Field
The invention relates to the field of metallurgy, in particular to a vanadium-aluminum alloy and a preparation method thereof.
Background
The thermite process is a process for obtaining a high-melting-point metal simple substance by utilizing the reducibility of aluminum. Thermite refers to a mixture of aluminum and metal oxide. Mixing aluminium powder with a certain amount of high-melting point metal oxide (such as iron oxide, etc.), igniting with magnesium strip, so that the aluminium powder can be seen to react violently at higher temperature, and a large amount of heat is released by the reaction, and a brilliant light is emitted. The product is alumina and the simple substance of the high melting point metal. Thermite reaction is very violent, so it is difficult to extinguish after ignition and to control the reaction process after ignition. The reaction is to charge the furnace burden, and to generate high temperature (1700 ℃ to 3000 ℃) quickly after ignition so that the furnace burden is in a molten state, and then alloy refining is carried out. The smelting method has the advantages of no need of electric heat input, low energy consumption and lower production cost than an electric arc furnace smelting method.
Vanadium-aluminium alloys are a basic raw material for titanium alloys and currently represent the second largest field of application following the application of vanadium in steel. The titanium alloy comprises Ti-6Al-4V and Ti-8Al-1Mo-1V, the total amount of the two titanium alloys accounts for 50% of the titanium alloy market, and the titanium alloy is mainly used for producing jet engines, high-speed aircraft frameworks and rocket engine casings. The vanadium used for producing the titanium alloy is added in the form of vanadium-aluminum alloy. Countries such as japan, the united states, the united kingdom and the like are also under further increasing research on the application of vanadium-titanium-containing alloys in the civil industry.
At present, vanadium pentoxide is generally used as a raw material in a vanadium-aluminum alloy production process, and a vanadium-aluminum alloy is produced by an aluminothermic method. Because vanadium pentoxide reacts with metal aluminum to release a large amount of heat, the heat is greatly excessive, the reaction is explosive, and the temperature of the system is sufficiently raised to over 3000 ℃ under the adiabatic condition. Therefore, a certain amount of inert material (commonly known as a heat dissipater) is usually added to the charge to control the reaction rate and the temperature rise of the reaction products. Because the heat-eliminating agent always contains a certain amount of Fe, Si, P and heavy metal elements, the produced vanadium-aluminum alloy has high impurity content.
Chinese patent application CN200910117560.4 discloses a preparation method of a vanadium-aluminum alloy material, which comprises the following steps of weighing powdery Al: 0% to 33.1%, V2O5: 50% -66.9% in a ball millAfter mixing for 8-16 hours, placing the mixture into a copper mold, compacting the mixture by using a press machine under the pressure of 60-80 MPa, placing the mold filled with the pressed reaction materials into an aluminothermic reaction container, placing an ignition agent on the materials, blowing out residual air by using inert gas, and heating the mixture to about 300 ℃ under the protection of argon gas of 2-7 MPa to react to obtain the vanadium-aluminum alloy, wherein the vanadium-aluminum alloy comprises 75-95% of V, 5.0-25.0% of Al, about 0.15% of S and about 0.50% of Fe by mass percent. Obviously, in the process, the obtained product has high content of impurities such as Fe, S and the like, because some impurities are introduced after the product is mixed in a ball mill for 8-16 hours. In addition, since the thermite reaction is performed in a closed pressure vessel, the production of vanadium-aluminum alloy is greatly limited, and further, since the pressure resistance of the equipment is required to be strong, the manufacturing cost is increased.
Disclosure of Invention
The invention aims to solve the problems of high impurity content, high manufacturing cost and low yield of vanadium-aluminum alloy in the prior art, and provides a vanadium-aluminum alloy and a preparation method thereof.
In order to achieve the above object, an aspect of the present invention provides a method for preparing a vanadium-aluminum alloy, the method comprising the steps of:
(1) mixing vanadium pentoxide and aluminum particles according to the weight ratio of (1.03-1.9) to 1 to obtain a mixture;
(2) paving part of the mixture at the bottom of a smelting furnace, igniting and igniting the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to perform aluminothermic reaction, and standing after the reaction is finished to obtain vanadium-aluminum alloy;
in the step (1), the purity of the aluminum pentoxide is more than or equal to 99.6 wt%, and the purity of the aluminum particles is more than or equal to 99.7 wt%.
Preferably, in step (2), the weight of the portion of the mix is 5-10% of the weight of the mix obtained in step (1).
Preferably, in the step (2), the ignition agent for igniting the ignition is barium peroxide and/or aluminum powder.
Preferably, in the step (2), the furnace body of the smelting furnace is a graphite crucible.
Preferably, in the step (2), the inner wall of the graphite crucible is coated with fused magnesia fire clay.
Preferably, in the step (2), the feeding speed of the continuous feeding is 10 to 50 kg/min.
Preferably, in the step (2), the feeding speed of the continuous feeding is 15 to 45 kg/min.
Preferably, in the step (2), the standing time is 72-96 h.
Preferably, in step (2), the ignition agent for igniting the ignition is magnesium strips.
The second aspect of the present invention provides a vanadium-aluminum alloy prepared by the above method, wherein the vanadium-aluminum alloy contains: 55.9-90.36 wt% of V, less than or equal to 0.10 wt% of Fe, less than or equal to 0.18 wt% of Si and the balance of Al.
Compared with the prior art, the preparation method provided by the invention has the advantages that the production scale can be enlarged by adopting a continuous feeding mode, the alloy ingot can be kept in a molten state for a longer time, and the yield of vanadium is improved. And conventional lime and other slagging coolants are not added to adjust heat, so that the cost is lower, the introduction of impurities can be reduced, the content of the impurities in the vanadium-aluminum alloy can be further reduced, and the purity of the obtained alloy is higher. According to the invention, the graphite crucible is adopted for smelting, the appearance quality of the prepared alloy is smoother and tidier than that of the alloy prepared by a knotting furnace body, the alloy quality is higher, higher yield can be obtained when the alloy cake is crushed, and the requirements of industrial mass production are completely met.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of a vanadium-aluminum alloy, which comprises the following steps:
(1) mixing vanadium pentoxide and aluminum particles according to the weight ratio of (1.03-1.9) to 1 to obtain a mixture;
(2) paving part of the mixture at the bottom of a smelting furnace, igniting and igniting the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to perform aluminothermic reaction, and standing after the reaction is finished to obtain vanadium-aluminum alloy;
in the step (1), the purity of the vanadium pentoxide is more than or equal to 99.6 wt%, and the purity of the aluminum particles is more than or equal to 99.7 wt%.
In the invention, excessive aluminum particles are adopted, part of aluminum reacts with vanadium pentoxide to generate metal vanadium and aluminum oxide in the reduction reaction process, at the moment, the vanadium pentoxide reacts, redundant aluminum and the generated metal vanadium form vanadium-aluminum alloy, and the vanadium-aluminum alloy with different vanadium-aluminum ratios can be formed according to the amount of the residual aluminum in the actual production process.
In a preferred embodiment, in step (2), the weight of the portion of the mix is 5 to 10% by weight of the mix obtained in step (1). Specifically, the weight of the partial mix may be 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, or 10 wt% of the mix obtained in step (1).
In a preferred embodiment, in step (2), the ignition agent for igniting the ignition is barium peroxide and/or aluminum powder.
In a preferred embodiment, in the step (2), the furnace body of the smelting furnace is a graphite crucible.
Further preferably, in the step (2), the inner wall of the graphite crucible is coated with fused magnesia fire clay.
In the invention, the graphite crucible is provided with the drilling cover, so that the alloy liquid can be prevented from splashing in the smelting process, and the heat preservation process is realized, thereby being beneficial to separating slag and gold. And the inner wall of the graphite crucible is coated with the fused magnesia fire clay coating, and proper smelting heat is configured in the smelting process, so that a coolant is not required to be added, other impurities are not introduced, and the vanadium-aluminum alloy with low impurity content can be obtained.
In a preferred embodiment, in step (2), the feeding rate of the continuous feeding is 10 to 50 kg/min. Specifically, the feeding speed can be 10kg/min, 15kg/min, 20kg/min, 25kg/min, 30kg/min, 35kg/min, 40kg/min, 45kg/min or 50 kg/min.
Further preferably, in the step (2), the feeding speed of the continuous feeding is 15 to 45 kg/min.
In a preferred embodiment, in the step (2), the standing time is 72 to 96 hours. Specifically, the standing time can be 72h, 74h, 76h, 78h, 80h, 82h, 84h, 86h, 88h, 90h, 82h, 94h or 96 h.
In a preferred embodiment, in step (2), the ignition aid for igniting the ignition is a magnesium strip.
The second aspect of the present invention provides a vanadium-aluminum alloy prepared by the above method, wherein the vanadium-aluminum alloy contains: 55.9-90.36 wt% of V, less than or equal to 0.10 wt% of Fe, less than or equal to 0.18 wt% of Si and the balance of Al.
Compared with the prior art, the preparation method provided by the invention has the advantages that the production scale can be enlarged by adopting a continuous feeding mode, the alloy ingot can be kept in a molten state for a longer time, and the yield of vanadium is improved. And conventional lime and other slagging coolants are not added to adjust heat, so that the cost is lower, the introduction of impurities can be reduced, the content of the impurities in the vanadium-aluminum alloy can be further reduced, and the purity of the obtained alloy is higher. According to the invention, the graphite crucible is adopted for smelting, the appearance quality of the prepared alloy is smoother and tidier than that of the alloy prepared by a knotting furnace body, the alloy quality is higher, higher yield can be obtained when the alloy cake is crushed, and the requirements of industrial mass production are completely met.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
Example 1
(1) 100kg of vanadium pentoxide (with a purity of 99.62 wt%) and 55.7kg of aluminum pellets (with a purity of 99.71 wt%) were mixed (the weight ratio of vanadium pentoxide to aluminum pellets was 1.795:1) to obtain a mixture;
(2) laying 7.79kg of the mixture at the bottom of a smelting furnace (a furnace body is a graphite crucible, and the inner wall of the furnace body is coated with fused magnesium fire mud), igniting the mixture by using analytically pure barium peroxide and using magnesium strips to ignite the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to perform aluminothermic reaction, wherein the feeding speed is 10kg/min, and standing for 72 hours after the reaction is finished to obtain 60.3kg of vanadium-aluminum alloy.
Example 2
(1) 200kg of vanadium pentoxide (having a purity of 99.7 wt%) and 127.4kg of aluminum pellets (having a purity of 99.73 wt%) were mixed (the weight ratio of vanadium pentoxide to aluminum pellets was 1.57:1) to obtain a mixture;
(2) laying 22.92kg of mixture at the bottom of a smelting furnace (a furnace body is a graphite crucible, and the inner wall of the furnace body is coated with fused magnesium fire mud), igniting the mixture by using analytically pure barium peroxide and using magnesium strips to ignite the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to carry out aluminothermic reaction, wherein the feeding speed is 15kg/min, and standing for 76h after the reaction is finished to obtain 127.52kg of vanadium-aluminum alloy.
Example 3
(1) 300kg of vanadium pentoxide (having a purity of 99.76 wt%) and 250.2kg of aluminum pellets (having a purity of 99.8 wt%) were mixed (the weight ratio of vanadium pentoxide to aluminum pellets was 1.2:1) to obtain a mixture;
(2) laying 44.01kg of mixture at the bottom of a smelting furnace (a furnace body is a graphite crucible, and the inner wall of the furnace body is coated with fused magnesium fire mud), igniting the mixture by using analytically pure barium peroxide and using magnesium strips to ignite the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to carry out aluminothermic reaction, wherein the feeding speed is 18kg/min, and standing for 80h after the reaction is finished to obtain 249.4kg of vanadium-aluminum alloy.
Example 4
(1) Mixing 400kg of vanadium pentoxide (with a purity of 99.81 wt%) and 384.61kg of aluminum particles (with a purity of 99.83 wt%) (the weight ratio of vanadium pentoxide to aluminum particles is 1.04:1) to obtain a mixture;
(2) laying 78.46kg of mixture at the bottom of a smelting furnace (a furnace body is a graphite crucible, and the inner wall of the furnace body is coated with fused magnesium fire mud), igniting the mixture by using analytically pure barium peroxide and using magnesium strips to ignite the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to carry out aluminothermic reaction, wherein the feeding speed is 46kg/min, and standing for 80h after the reaction is finished to obtain 394.3kg of vanadium-aluminum alloy.
Comparative example 1
The procedure was followed as described in example 1, except that in step (2), the remaining mix was added in a single addition to give 59.7kg of a vanadium-aluminium alloy.
Comparative example 2
The procedure is as described in example 4, except that the amount of aluminium particles used is 400kg, i.e. the weight ratio of vanadium pentoxide to aluminium particles is 1:1, giving 411.69kg of vanadium-aluminium alloy.
Test example
The chemical compositions of the vanadium-aluminum alloys prepared in the examples and the test examples were detected by a chemical analysis method, and the vanadium yield was calculated, with the results shown in table 1.
TABLE 1
Figure BDA0003277211230000071
Figure BDA0003277211230000081
The results in table 1 show that the method of the present invention can successfully prepare vanadium-aluminum alloy with low impurity content and high vanadium yield.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (10)

1. The preparation method of the vanadium-aluminum alloy is characterized by comprising the following steps of:
(1) mixing vanadium pentoxide and aluminum particles according to the weight ratio of (1.03-1.9) to 1 to obtain a mixture;
(2) paving part of the mixture at the bottom of a smelting furnace, igniting and igniting the mixture, adding the rest mixture in a continuous feeding mode after the mixture starts to perform aluminothermic reaction, and standing after the reaction is finished to obtain vanadium-aluminum alloy;
in the step (1), the purity of the aluminum pentoxide is more than or equal to 99.6 wt%, and the purity of the aluminum particles is more than or equal to 99.7 wt%.
2. The method for preparing the vanadium-aluminum alloy according to claim 1, wherein in the step (2), the weight of the part of the mixed material is 5-10 wt% of the mixed material obtained in the step (1).
3. The method for preparing the vanadium-aluminum alloy according to claim 1 or 2, wherein in the step (2), the ignition agent for igniting the ignition is barium peroxide and/or aluminum powder.
4. The method for preparing the vanadium-aluminum alloy according to claim 1, wherein in the step (2), the furnace body of the smelting furnace is a graphite crucible.
5. The method for preparing the vanadium-aluminum alloy according to claim 4, wherein in the step (2), the inner wall of the graphite crucible is coated with the fused magnesia fire clay.
6. The method for preparing the vanadium-aluminum alloy according to claim 1, wherein in the step (2), the feeding speed of the continuous feeding is 10 to 50 kg/min.
7. The method for preparing the vanadium-aluminum alloy according to claim 6, wherein in the step (2), the feeding speed of the continuous feeding is 15 to 45 kg/min.
8. The method for preparing the vanadium-aluminum alloy according to claim 1, wherein in the step (2), the standing time is 72 to 96 hours.
9. The method for preparing the vanadium-aluminum alloy according to claim 1, wherein in the step (2), the ignition agent for igniting is a magnesium strip.
10. The vanadium-aluminum alloy produced by the method of any one of claims 1 to 9, wherein the vanadium-aluminum alloy comprises: 55.9-90.36 wt% of V, less than or equal to 0.10 wt% of Fe, less than or equal to 0.18 wt% of Si and the balance of Al.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115627400A (en) * 2022-10-11 2023-01-20 散裂中子源科学中心 Light vanadium-aluminum alloy for neutron scattering experiments and preparation method and application thereof

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CN108330370A (en) * 2018-03-20 2018-07-27 攀钢集团研究院有限公司 A kind of production method of vananum

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JPS6277432A (en) * 1985-09-30 1987-04-09 Nippon Kokan Kk <Nkk> Manufacture of v-al alloy containing 60-90% v and 40-10% al
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115627400A (en) * 2022-10-11 2023-01-20 散裂中子源科学中心 Light vanadium-aluminum alloy for neutron scattering experiments and preparation method and application thereof
CN115627400B (en) * 2022-10-11 2023-10-13 散裂中子源科学中心 Light vanadium-aluminum alloy for neutron scattering experiment and preparation method and application thereof

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Application publication date: 20220121